Method for preparing salvianolic acid B through separation by means of flash chromatography

A chromatographic separation and salvianolic acid technology, applied in organic chemistry and other directions, can solve the problems of difficult production and storage of traditional Chinese medicine preparations, high requirements for equipment and reagents, and difficulty in large-scale production. Degradation reduction effect

Inactive Publication Date: 2014-05-14
SUN YAT SEN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the stability of salvianolic acid B in aqueous solution has a great relationship with pH value and temperature, which brings great difficulties to the production and storage of traditional Chinese medicine preparations.
[0003] At present, the separation and purification methods of salvianolic acid B mainly include: (1) column chromatography, but the operation is more complicated, the efficiency is not high, and different fillers are required to be used in combination; Reagent requirements are high, the cost is high, and it is difficult to produce on a large scale; (3) high-speed countercurrent chromatography requires a large number of experiments to select a suitable solvent system

Method used

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  • Method for preparing salvianolic acid B through separation by means of flash chromatography
  • Method for preparing salvianolic acid B through separation by means of flash chromatography
  • Method for preparing salvianolic acid B through separation by means of flash chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0039] 1. Medicinal material processing

[0040] Take Danshen decoction pieces, crush them, take 15g and add 50% ethanol by volume fraction at a ratio of 1:20 (m / v), soak for 6 hours, sonicate for 1 hour, filter, and add 50% ethanol by volume fraction at a ratio of 1:20 (m / v) to the residue Extract again for 1h and filter. Combine the filtrates extracted twice, concentrate under reduced pressure to 1 / 4 of the original volume, filter, and extract the filtrate 3 times with diethyl ether volume ratio (1:1), add 1mol L -1 Adjust the pH to 3 with HCl, filter, and extract the filtrate 3 times with ethyl acetate in a volume ratio (1:1), combine the ethyl acetate layers, and concentrate to dryness under reduced pressure to obtain ethyl acetate extract (0.65 g).

[0041] 2. Sample Processing

[0042] Take 100mg of ethyl acetate extract, add 25% volume fraction of methanol water and dissolve it to prepare a concentration of 30mg·mL -1 The solution was centrifuged for 10min (15000rpm)...

Embodiment 2

[0057] 1. Medicinal material processing

[0058] Take Danshen decoction pieces, crush them, take 15g, add 50% ethanol by volume fraction at a ratio of 1:20 (m / v), soak for 6 hours, ultrasonicate for 1 hour, filter, and add 50% ethanol by volume fraction at a solid-liquid ratio of 1:20 to extract again ,filter. Combine the filtrates extracted twice, concentrate under reduced pressure to 1 / 4 of the original volume, filter, and extract the filtrate 3 times with diethyl ether volume ratio (1:1), add 1mol L -1 HCl was adjusted to pH = 4, filtered, and the filtrate was extracted three times with ethyl acetate in a volume ratio (1:1). The ethyl acetate layers were combined and concentrated to dryness under reduced pressure to obtain ethyl acetate extract (0.62 g).

[0059] 2. Sample Processing

[0060] Take 120mg of ethyl acetate extract, add 25% volume fraction of methanol water and dissolve it to prepare a concentration of 60mg·mL -1 The solution was centrifuged for 10min (15000...

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Abstract

The invention provides a method for preparing salvianolic acid B through separation by means of flash chromatography, which is a preparation method for separating out and purifying the salvianolic acid B with purity higher than 98.0 percent from salvia miltiorrhiza as medicinal material. After the medicinal material is extracted and extracted with organic solvent, ethyl acetate extract is obtained, and with methanol-water as an elution system, a flash chromatograph and a medium / low pressure chromatographic column with C18 bonded phase as packing material are adopted to automatically collect eluent. The eluent is extracted with organic solvent, depressurized to be concentrated and dried under vacuum, and finally, the salvianolic acid B with purity higher than 98.0 percent is obtained. Compared with the prior art, the method is easy to operate, the cost is low, the repeatability is good, the efficiency is high, the product purity is high, and the method can be used for the mass production of the salvianolic acid B.

Description

technical field [0001] The invention relates to a method for preparing salvianolic acid B with a purity greater than 98.0% obtained by separating and purifying salvia miltiorrhiza. technical background [0002] Salvia miltiorrhiza is the dry root and rhizome of Salvia miltiorrhiza Bge., a plant in the Labiatae family. It has the effects of dispelling stasis and relieving pain, promoting blood circulation and stimulating menstruation, clearing heart and eliminating troubles. Salvia mainly contains two types of active ingredients: one is fat-soluble diterpenoids, and the other is water-soluble polyphenolic acids. Experimental studies have proved that the water-soluble components of Danshen have various pharmacological activities and have strong antioxidant activity. Salvianolic acid B is one of the important water-soluble active ingredients in Danshen, accounting for about 70% of the total phenolic acids. In the 2010 edition of the Chinese Pharmacopoeia, salvianolic acid B ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/86
Inventor 徐新军谢春燕谢鸷生黄洁云杨梅王建王大冲
Owner SUN YAT SEN UNIV
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